Classifications

• • B—PERFORMING OPERATIONS; TRANSPORTING
  • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
  • B01D—SEPARATION
  • B01D53/00—Separation of gases or vapours; Recovering vapours of volatile solvents from gases; Chemical or biological purification of waste gases, e.g. engine exhaust gases, smoke, fumes, flue gases, aerosols
  • B01D53/02—Separation of gases or vapours; Recovering vapours of volatile solvents from gases; Chemical or biological purification of waste gases, e.g. engine exhaust gases, smoke, fumes, flue gases, aerosols by adsorption, e.g. preparative gas chromatography
• • B—PERFORMING OPERATIONS; TRANSPORTING
  • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
  • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
  • B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
  • B01J20/28—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof characterised by their form or physical properties
  • B01J20/28054—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof characterised by their form or physical properties characterised by their surface properties or porosity
  • B01J20/28057—Surface area, e.g. B.E.T specific surface area
• • B—PERFORMING OPERATIONS; TRANSPORTING
  • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
  • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
  • B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
  • B01J20/30—Processes for preparing, regenerating, or reactivating
  • B01J20/305—Addition of material, later completely removed, e.g. as result of heat treatment, leaching or washing, e.g. for forming pores
• • B—PERFORMING OPERATIONS; TRANSPORTING
  • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
  • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
  • B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
  • B01J20/30—Processes for preparing, regenerating, or reactivating
  • B01J20/3078—Thermal treatment, e.g. calcining or pyrolizing
• • B—PERFORMING OPERATIONS; TRANSPORTING
  • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
  • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
  • B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
  • B01J20/30—Processes for preparing, regenerating, or reactivating
  • B01J20/3085—Chemical treatments not covered by groups B01J20/3007 - B01J20/3078
• • B—PERFORMING OPERATIONS; TRANSPORTING
  • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
  • B01D—SEPARATION
  • B01D2253/00—Adsorbents used in seperation treatment of gases and vapours
  • B01D2253/10—Inorganic adsorbents
• • B—PERFORMING OPERATIONS; TRANSPORTING
  • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
  • B01D—SEPARATION
  • B01D2257/00—Components to be removed
  • B01D2257/50—Carbon oxides
  • B01D2257/504—Carbon dioxide
• • B—PERFORMING OPERATIONS; TRANSPORTING
  • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
  • B01D—SEPARATION
  • B01D2259/00—Type of treatment
  • B01D2259/40—Further details for adsorption processes and devices
  • B01D2259/40083—Regeneration of adsorbents in processes other than pressure or temperature swing adsorption
  • B01D2259/40088—Regeneration of adsorbents in processes other than pressure or temperature swing adsorption by heating
  • B01D2259/4009—Regeneration of adsorbents in processes other than pressure or temperature swing adsorption by heating using hot gas
• • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
  • Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
  • Y02C—CAPTURE, STORAGE, SEQUESTRATION OR DISPOSAL OF GREENHOUSE GASES [GHG]
  • Y02C20/00—Capture or disposal of greenhouse gases
  • Y02C20/40—Capture or disposal of greenhouse gases of CO2

Definitions

• the present invention relates to a method of treating a gas to reduce its carbon dioxide content.
• CO2 carbon dioxide
• the object of the invention is to provide such a compound.
• the process of the invention for treating a gas to reduce its carbon dioxide content is characterized in that the gas is brought into contact with a compound of at least one rare earth by which the carbon dioxide is adsorbed on the compound and a gas depleted of carbon dioxide is obtained.
• the use of a rare earth compound has the advantage of allowing in particular a maximum of the release of the adsorbed CO 2 at a temperature which may be less than 300 ° C. and even at most 250 ° C. and in addition in a range of more limited temperature than in the case of the processes of the prior art, that is to say a range whose amplitude may be less than 300 0 C.
• For rare earth is meant for the remainder of the description the elements of the group consisting of yttrium and the elements of the periodic classification of atomic number inclusive between 57 and 71.
• specific surface is meant the specific surface B. AND. determined by nitrogen adsorption according to ASTM D 3663-78 established from the BRUNAUER-EMMETT-TELLER method described in the journal "The Journal of the American Chemical Society, 60, 309 (1938)".
• the calcinations at which the surface values are given are calcinations under air.
• the specific surface values given for a given temperature and duration correspond, unless otherwise indicated, to calcinations at a temperature step over the indicated time.
• the main feature of the invention is the use of a rare earth compound for capturing or adsorbing the CO 2 contained in the gas to be treated.
• This compound may be based on an oxide, an oxyhydroxide, a nitrate or a carbonate.
• the term oxide when used on the subject of the rare earth compound means not only in the sense of oxide but also in the sense of carbonate oxide because often the oxides can carbonate by simple contact with air and they may also contain nitrates.
• This treatment can be done by heating under a gas flow, especially air, which air can contain steam at temperatures greater than or equal to those used in the process for regenerating the material after storage of CO 2 .
• the temperature will be as low as possible, typically less than 500 ° C., preferably less than 300 ° C.
• the compound is based on at least one rare earth chosen from cerium, lanthanum or praseodymium.
• This embodiment applies more particularly to the case where the compound is in oxide form. Mention may more particularly be made of cerium and lanthanum, cerium and praseodymium-based compounds, or else based on cerium, lanthanum and praseodymium, these elements being even more particularly in the form of an oxide in the compound.
• a compound of at least one rare earth which additionally contains zirconium.
• This compound may contain one or more rare earths.
• cerium and zirconium compounds based on cerium and zirconium may be mentioned in particular. and praseodymium, based on cerium, zirconium and lanthanum or based on cerium, zirconium, praseodymium and lanthanum.
• the compounds may be more particularly based on the oxides of the elements mentioned (cerium, zirconium and other rare earths).
• the proportion of cerium may in particular be at least 50% and more particularly of at least 70%, this proportion being expressed in cerium oxide equivalent CeO2 relative to the total weight, in the compound, of cerium and of the other element or elements expressed as oxide.
• the cerium content may be even more particularly at least 80% or even at least 90%.
• the proportion (expressed as above) of rare earth other than cerium or zirconium is usually at least 0.5%, more particularly at least 1%.
• is used in the process of the invention is a compound of at least one rare earth that further contains zirconium or a compound of at least two rare earths, this compound then occurring in the form of a solid solution.
• solid solution is meant that the X-ray diffraction patterns of the compounds reveal, within them, the existence of a single homogeneous phase.
• this phase corresponds in fact to that of a ceric oxide CeO 2 crystallized and whose mesh parameters are more or less staggered with respect to a pure ceric oxide, thus reflecting the incorporation the other element, zirconium or rare earth, in the crystal lattice of cerium oxide, and thus obtaining a true solid solution.
• compounds whose specific surface area is important.
• some examples of the compounds which can be used in the present invention will be given below. .
• cerium oxides with a stabilized surface area can be used in particular.
• cerium oxides which have a high specific surface even after being exposed to high temperatures can be used in particular.
• cerium oxide described in EP-A-300852 which has a specific surface area of at least 15 m 2 / g after calcination at a temperature of between 800 ° C. and 900 ° C. for at least 2 hours or still the cerium oxide described in EP-A-388567 which has an area of at least 190 m 2 / g after calcination at a temperature between 350 ° C and 450 ° C for at least 2 hours with furthermore a specific surface area of at least 15 m 2 / g after calcination at a temperature of between 800 ° C. and 900 ° C. for the same duration.
• the oxides which have been described in the above paragraphs may have advantageously underwent a new calcination at 500 ° C. under air before being used.
• compositions based on a cerium oxide and a zirconium oxide and more particularly compositions for which there is a cerium / zirconium atomic proportion of at least 1.
• cerium oxide described in EP-A-207857 which has a specific surface greater than 10 m 2 / g up to a temperature of 900 ° C.
• This oxide can present in particular a content of oxide of zirconium between 1 and 20% relative to the weight of the ceric oxide.
• the composition based on cerium oxide and zirconium oxide which is the subject of EP-A-605274 and in which the zirconium is in solid solution in cerium oxide.
• This composition may have a specific surface area of at least 30 m 2 / g after calcination at 800 ° C. for 6 hours.
• compositions of the type based on a cerium oxide and a zirconium oxide and at least one oxide chosen from rare earth oxides other than cerium are in particular described in EP-A-906244.
• compositions have a cerium / zirconium atomic proportion of at least 1 and a specific surface area of at least 35 m 2 / g after calcination for 6 hours at 900 ° C.
• This surface may be more particularly at least 40 m 2 / g. It may be even more particularly at least 45 m 2 / g.
• These compositions are prepared by a process in which a mixture is prepared in a liquid medium containing a cerium compound, a zirconium compound, which may be in particular a zirconyl nitrate obtained by nitric attack of a zirconium carbonate, and a compound of rare earth; said mixture is heated; the precipitate obtained is recovered and this precipitate is calcined.
• the starting mixture is prepared using a solution of zirconium which is such that the amount of base necessary to reach the equivalent point during an acid-base assay of this solution satisfies the condition molar ratio OH7Zr ⁇ 1.65.
• Usable compounds are also those based on a cerium oxide and a praseodymium oxide and for which the proportion of praseodymium may range up to a mass ratio expressed as praseodymium oxide relative to the cerium oxide of 50%. This proportion is usually at least 0.5%. This proportion can thus be between 1 and 40%, especially between 1 and 20%, more particularly between 1 and 10%.
• the composition may further comprise zirconium. Compositions of this type are described in FR 2729309 A1 and which, after calcination for 6 hours at 400 ° C., have a specific surface area of at least 10 m 2 / g, preferably at least 60 m 2 / g and more particularly at least 80 m 2 / g.
• cerium, zirconium and possibly at least one other rare earth-based compounds which have been described above and for which the concentrations of cerium and of rare earth are different at the surface and at the compounds, such products can be obtained by impregnation with a solution comprising a cerium optionally rare earth, a compound based on cerium, zirconium and rare earth if necessary, previously prepared according to the teaching of one of the patent applications mentioned above.
• compositions based on cerium oxide and at least one oxide of another rare earth which have the characteristic of presenting surfaces. particularly high since this is at least
• compositions of this particular embodiment consist essentially of cerium oxide and one or more oxides of a rare earth.
• the compositions may contain elements such as impurities that may notably come from its preparation process, for example starting materials or starting reagents used.
• the rare earth may be more particularly yttrium, neodymium, lanthanum or praseodymium. According to one variant, lanthanum and praseodymium are present in combination in the composition.
• the content of rare earth oxide is generally at most 25%, preferably when the rare earth is lanthanum, more particularly at most 20% and preferably at most 15% by weight.
• the minimum content is not critical but generally it is at least 1%, more preferably at least 2% and preferably at least 5% by weight. This content is expressed as the oxide of the rare earth relative to the mass of the entire composition.
• the compositions of this particular embodiment of the invention may furthermore have a surface area of at least 22 m 2 / g after calcination at 1000 ° C. for 5 hours. More generally, values of at least about 25 m 2 / g can be obtained under the same calcination conditions.
• the specific surfaces of the compositions of this particular embodiment of the invention may still be high even at an even higher temperature. Thus, these surfaces can be from to minus 10 m 2 / g, more particularly at least 14 m 2 / g after calcination at 1100 ° C. for 5 hours.
• compositions of this embodiment may have a specific surface area of at least 30 m 2 / g after calcination at 900 ° C. for 5 hours. More generally, values of at least about 35 m 2 / g can be obtained under the same calcination conditions.
• compositions are prepared by a specific method which will now be described.
• This process is characterized in that it comprises the following steps: a liquid medium comprising a cerium compound is formed;
• the medium is heated to a temperature of at least 100 ° C .
• the precipitate obtained at the end of the preceding stage is separated from the liquid medium, a compound of the other rare earth is added thereto and another liquid medium is formed; the medium thus obtained is heated to a temperature of at least 100 ° C.
• reaction medium obtained at the end of the preceding heating is brought to a basic pH
• the first step of the process therefore consists in forming a liquid medium comprising a cerium compound.
• the liquid medium is usually water.
• the cerium compound is preferably selected from soluble compounds. It may be in particular an organic or inorganic acid salt such as a nitrate, a sulfate, an acetate, a chloride, a cerium-ammoniacal nitrate.
• ceric nitrate is used. It is advantageous to use salts of purity of at least 99.5% and more particularly at least
• An aqueous solution of ceric nitrate may, for example, be obtained by reacting nitric acid with a hydrated ceric oxide prepared in a conventional manner by reacting a solution of a cerous salt, for example cerous nitrate, and an ammonia solution in the presence of hydrogen peroxide. It is also preferable to use a solution of ceric nitrate obtained by the electrolytic oxidation method of a cerous nitrate solution as described in document FR-A-2 570 087, and which constitutes here an interesting raw material. .
• aqueous solutions of cerium salts may have some initial free acidity which can be adjusted by the addition of a base or an acid. It is however as possible to implement an initial solution of cehum salts actually having a certain free acidity as mentioned above, than solutions which have previously been neutralized more or less extensively.
• This neutralization can be done by adding a basic compound to the aforementioned mixture so as to limit this acidity.
• This basic compound may be for example a solution of ammonia or alkali hydroxides (sodium, potassium, etc.), but preferably an ammonia solution.
• the starting mixture contains céhum essentially in form III
• an oxidizing agent for example hydrogen peroxide
• a soil as the starting compound of cerium.
• sol any system consisting of fine solid particles of colloidal dimensions, ie dimensions of between about 1 nm and about 500 nm, based on a cerium compound, this compound being generally an oxide and / or an oxide hydrated cerium, suspended in an aqueous liquid phase, said particles may further possibly contain residual amounts of bound or adsorbed ions such as for example nitrates, acetates, chlorides or ammoniums.
• the cerium can be either totally in the form of colloids, or simultaneously in the form of ions and in the form of colloids.
• the mixture can be indifferently obtained either from compounds initially in the solid state that will be introduced later in a water tank for example, or even directly from solutions of these compounds.
• the second step of the process consists in heating the medium prepared in the preceding step to a temperature of at least 100 ° C.
• the temperature at which the medium is heated is generally between 100 ° C. and 150 ° C., more particularly between 110 ° C. and 130 ° C.
• the heating operation can be conducted by introducing the liquid medium into a closed chamber (autoclave type closed reactor). Under the conditions of the temperatures given above, and in aqueous medium, it is thus possible to specify, by way of illustration, that the pressure in the closed reactor can vary between a value greater than 1 bar (10 5 Pa) and 165 bar (1 bar). , 65. 10 7 Pa), preferably between 5 Bar (5 ⁇ 10 5 Pa) and 165 Bar (1, 65. 10 7 Pa). It is also possible to carry out heating in an open reactor for temperatures close to 100 ° C. The heating may be conducted either in air or in an atmosphere of inert gas, preferably nitrogen.
• the duration of the heating can vary within wide limits, for example between 30 minutes and 48 hours, preferably between 1 and 5 hours.
• the rise in temperature is carried out at a speed which is not critical, and it is thus possible to reach the reaction temperature set by heating the medium for example between 30 minutes and 4 hours, these values being given for all purposes. indicative fact.
• a precipitate is obtained which is separated from the liquid medium by any suitable means, for example by withdrawing the mother liquors.
• a compound of the other rare earth forming a second liquid medium.
• the rare earth compound may be of the same nature as the cerium compound used in the first step of the process. What has been described above for this compound therefore applies here to the rare earth compound which may be more particularly chosen from nitrates, sulphates, acetates, chlorides.
• the second liquid medium is heated to a temperature of at least 100 ° C. Again, what has been described above for the first heating also applies here for the second heating.
• the reaction medium obtained is brought to a basic pH.
• a basic compound is introduced into the reaction medium. Hydroxide products can be used as base or basic compound. Mention may be made of alkali or alkaline earth hydroxides.
• amines and ammonia may be preferred in that they reduce the risk of pollution by alkaline or alkaline earth cations.
• urea may be preferred in that they reduce the risk of pollution by alkaline or alkaline earth cations.
• the basic compound may more particularly be used in the form of a solution.
• the pH value at which the medium is brought may be more particularly between 8 and 10, more particularly between 8 and 9.
• the precipitate recovered is then calcined.
• This calcination makes it possible to develop the crystallinity of the product formed and it can also be adjusted and / or chosen as a function of the temperature of subsequent use reserved for the composition of this particular embodiment of the invention, and this taking into account the fact that the specific surface of the product is even lower than the calcination temperature implementation is higher.
• Such calcination is generally performed under air, but a calcination carried out for example under inert gas or under a controlled atmosphere (oxidizing or reducing) is obviously not excluded.
• the calcination temperature is generally limited to a range of values of between 300 ° C. and 1000 ° C.
• the process of the invention can be used for the treatment of any type of gas containing CO2.
• gases produced by industrial installations in which the combustion of hydrocarbons, coal or any fuel producing CO2 such as boilers or gas turbines is carried out. It may also be gases from petrochemical refining processes such as those from catalytic cracking units or gases from cement plants. Finally, the process of the invention can also be used for gases produced by domestic installations such as gas or fuel boilers.
• gases may comprise, for example, between 50% to 80% of nitrogen, between 5% to 20% of carbon dioxide (CO 2 ), between 2% to 10% of oxygen (O 2 ), and possibly other impurities such as SOx, NOx, dust or other particles.
• These gases may have a temperature ranging from ambient temperature (that is to say between 15 ° C. and 25 ° C.) and 850 ° C., in particular between 40 ° C. and 500 ° C., these temperatures not being limiting and given only by way of example only.
• ambient temperature that is to say between 15 ° C. and 25 ° C.
• 850 ° C. in particular between 40 ° C. and 500 ° C., these temperatures not being limiting and given only by way of example only.
• the gas treatment is done by bringing them into contact with the rare earth compound described above. This contacting can be done in a reactor specially provided for it or in an exchanger or a compressor or possibly any other apparatus of an installation through which the gases pass.
• the compound must have been shaped.
• the shaped compound may further comprise a binder.
• This binder is chosen from those which are usually used in extrusion techniques, for example silica, alumina, boehmite, clays, silicates, silico-aluminates, titanium sulphate, ceramics. These binders are present in the proportions generally used, that is to say up to about 30%, more particularly at most about 15% by weight.
• the compound may also be in the form of a coating on a ceramic or metal substrate or on the internal of the reactor: walls, distribution trays or internals of an exchanger, a compressor or any apparatus in which can pass the gas to be treated.
• the process of the invention may comprise a complementary carbon dioxide desorption stage of the rare earth compound at the end of which the carbon dioxide is recovered. This desorption can be done by passing a hot gas on this compound. This gas may be for example natural gas or air.
• the temperature of the hot gas is that which allows efficient desorption of CO 2 .
• An important advantage of the invention is that the temperature of this gas can be low.
• the temperature of this gas may especially be at most 350 ° C., more particularly at most 300 ° C. and even more particularly at most 250 ° C.
• This example concerns the preparation of compounds based on rare earths that can be used in the process of the invention
• This example illustrates the preparation of the mixed oxide of formula CeO 2 -ZrO 2 -Pr 6 having the composition of Table 1 and obtained by a process of the type described in EP-A-906244 mentioned above and to which refer.
• the OHVZr molar ratio corresponds to the amount of base that must be added to reach the equivalent point during the acid base assay of the zirconyl nitrate solution.
• This mixture (expressed as the oxide of the various elements) is then adjusted to 80 g / l. This mixture is then heated at 150 ° C. for 4 hours.
• This example illustrates the preparation of the mixed oxide of formula CeO 2 - La 2 O 3 -Pr 6 having the composition of Table 1.
• This example illustrates the preparation of the mixed oxide of formula CeO 2 -ZrO 2 -La 2 O 3 having the composition of Table 1.
• the procedure is the same as that of Example 1 -A, lanthanum nitrate being added in place of praseodymium nitrate.
• This example relates to the preparation of a compound containing an alkaline earth element known for storing CO 2 .
• a solution containing 4.10 g of barium nitrate (Prolabo Rectapur 99%) and 17.5 g of demineralized water is heated to 80 ° C.
• the impregnated alumina is then dried at 100 ° C. for 3 hours. This procedure is repeated a second time with the same amount of the barium nitrate solution. The alumina thus obtained is dried at 100 ° C. for
• the powder obtained is calcined in air at 500 ° C. for 2 hours.
• the compound 2-E thus obtained contains 80% by weight of alumina and 20% by weight of barium oxide BaO. It has a specific surface area of 81 m 2 / g.
• This example gives a comparison of the CO 2 release temperatures adsorbed on the various compounds of the preceding examples.
• the adsorption of CO2 was carried out under the following conditions. A 10% CO 2 synthetic gas is then passed into the air for 1 hour at a rate of 11 / h at room temperature over 10 g of each of the compounds 1-A to 2-E.
• the gravimetric thermal analysis (ATG) technique is used which consists in heating approximately 20 mg of each of the compounds of the preceding examples, weighed precisely, under a synthetic air stream at the rate of 30 ml / min.
• An increase in temperature is applied between ambient temperature and 700 0 C at an increase of 10 ° C / min which causes the release of CO2 and remission of CO2 in the gas output device.
• the CO2 content of the gas leaving the apparatus is determined by mass spectrometry.
• Table 2 compares the CO2 departure temperature window, characterized by a minimum temperature at which CO2 is emitted and a final temperature at which the CO2 emission stops. Between these two temperatures CO2 is emitted continuously. It also mentions the temperature called maximum temperature which corresponds to the temperature at which the maximum CO2 is emitted.
• the four compounds according to the invention containing cerium, optionally zirconium, lanthanum and / or praseodymium (1-A to 1 -D) lead to a release of CO 2 over a smaller range of temperature, generally between 50 and 250 ° C, while the comparative compound (2-E) leads to a CO 2 emission on a wider window, especially up to 630 0 C.
• the maximum CO 2 release temperature is also lower on compounds 1-A to 1-D: 100 at 120 ° C against 240 ° C for the compound 2-E.

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